CN101360680A - Method of forming a sealed channel of a microfluidic reactor and a microfluidic reactor comprising such channel - Google Patents
Method of forming a sealed channel of a microfluidic reactor and a microfluidic reactor comprising such channel Download PDFInfo
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- CN101360680A CN101360680A CNA2006800516610A CN200680051661A CN101360680A CN 101360680 A CN101360680 A CN 101360680A CN A2006800516610 A CNA2006800516610 A CN A2006800516610A CN 200680051661 A CN200680051661 A CN 200680051661A CN 101360680 A CN101360680 A CN 101360680A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
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- B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
- B81C1/00436—Shaping materials, i.e. techniques for structuring the substrate or the layers on the substrate
- B81C1/00444—Surface micromachining, i.e. structuring layers on the substrate
- B81C1/0046—Surface micromachining, i.e. structuring layers on the substrate using stamping, e.g. imprinting
Abstract
In a method according to the invention for forming a sealed channel (125) in the surface of a sheet made of a material with certain extent of plasticity, the machining surface of a tool with a rolling machining surface is brought into contact with a first point of the channel (125) to be formed in the surface of the sheet constituting a reactor block. Next, said machining surface is pressed onto the surface of the sheet with a compressive force (F) required to achieve the depth of the channel (125) to be formed, whereby the plastic material is squeezed out and becomes raised from the sheet surface on the peripheries of the depression being formed. After this, while maintaining the compressive force (F), by displacing said machining surface along the centerline of the channel (125) over the sheet surface it is rolled from the first point of the channel (125) to be formed to a second point thereof, whereby the channel (125) is machined in the material of the sheet and sealing edges (127) are created on the peripheries of the channel (125) from the material squeezed out and become raised. After creating said sealing edges (127), a closing member bearing against the sealing edges (127) is arranged at the surface of the sheet provided with the channel (125) and the sealing edges (127), and then said closing member is pressed onto the sheet by a compressive force required to deform said sealing edges (127) and is fixed in the position obtained, whereby a sealed channel (125) running between the first and second points is formed within the reactor block.
Description
Technical field
The present invention relates to a kind ofly form the seal channel method at the sheet surface of being made by the material with plasticity to a certain degree, described thin slice is formed for the reactor module of micro-fluidic reactor.The invention still further relates to a kind of micro-fluidic reactor, it comprises the seal channel that has export and import and be used to provide the chemical reaction space, described export and import all is communicated with the external environment condition of reactor, wherein, reactor comprises that also coupled mechanism keeps and first and second limited parts, closure member that is clamped together and the cooling chamber that is communicated with the reactor external environment condition, has a temperature conditioning unit in the described cooling chamber.
Background technology
In chemical industry, the reactor of large-size is used to carry out different types of plant-scale chemical reaction.Yet,, be used to laboratory scale experiment than the little a lot of flask of those reactor sizes for same purpose.Under many circumstances, with a small amount of and to produce the product of wishing at short notice be preferred---for example in reaction optimizing phase of research work.So-called micro-fluidic reactor can be counted as the laboratory reaction device for this purpose.
In the prior art, term " micro-fluidic reactor " is often referred to the seal channel that is provided with import and outlet and is used to hold the reactant mixture of the continuous or intermittent flow that temporarily stops with short time, wherein, described channel vertical is no more than 0.5mm in the size of the flow direction of reactant mixture.In micro-fluidic reactor, the flow rate of the length of passage and area of section and reactant mixture is selected as follows: it is sufficient that the time that the passage reaction mixture is spent (being called the time of staying from now on) finishes for desired response.The process of reaction or even its postpone to be subjected to usually the influence of external heating or cooling.Therefore, micro-fluidic reactor is equipped with external heat/cooling infrastructure usually.In addition, in great majority are used, micro-fluidic reactor by suitable structural change be adapted to can the hybrid reaction mixture component (reactant)---for example by equipping the mixed cell of suitable integral type for it.In order to regulate the flow rate by import, the pattern of flow of micro-fluidic reactor reaction mixture can be selected as laminar flow or turbulent flow.In addition, reactant is infeeded passage and product is discharged from passage by auxiliary the finishing of suitable connector is installed in import and outlet.If the reactant that reaction needed is a large amount of, that is, in the time will producing a large amount of product, a plurality of reactor unit fluids are parallel to be connected, thereby has improved production capacity in other benefit that keeps micro-fluidic reactor.U.S. patent application No.2003/0003024A1 discloses such micro-fluidic reactor.
The mixing of reactant in micro-fluidic reactor be because the shape of available flow path and little area of section and very effective, and therefore, the fluctuation of the local concentration of the reactant in the reactant mixture is minimum or can ignore in practice.By vapor-phase reactant is mixed in micro-fluidic reactor with the liquid phase reactor thing, selectively (promptly in diffusion controlled reaction) adds little bubble and drop simultaneously, can realize the high ratio of phase border surface and channel volume, this has positive role for reaction process.In addition, because the high ratio of phase border surface and channel volume, the effective temperature of reactant mixture can be controlled rapidly and effectively, and therefore, if desired, ongoing reaction can be simply by applying quick cooling " being freezed ".But if wish to realize exothermic reaction in micro-fluidic reactor, then the beginning of undesirable extra reaction can be prevented from owing to discharging the heat that produces fast and effectively simply.Use another advantage of micro-fluidic reactor to be that the temperature of reactant mixture and the time of staying can be changed any time during reaction immediately, therefore, at any time, can set the peak optimization reaction condition that is used for course of reaction.Correspondingly, the reaction of carrying out by this way can cause than produce greater amount and purer product in the reaction of carrying out when not having optimal conditions.At last, because less relatively channel cross-sectional area and change the ability of temperature fast, reliably also can be carried out other explosive chemical reaction with high level of security.
Present normally used micro-fluidic reactor is made by having high mechanical properties and erosion-resisting metal or glass (silica (silica)).The passage that is used for holding reactant mixture forms on the surface of the so-called reactor module of being made by described metal or glass.Described formation is for example undertaken by photoetching process or chemical ion etching under the situation of glass, and for example under the situation of metallic reactors module, undertaken by machined and/or die forging method, as for example at U.S. patent application No.2003/0003024 A1 and EP-1, that describes in detail among 473,077 A2 is such.Subsequently, the passage that forms in reactor module is covered by the closure member made from the reactor module identical materials usually, and reactor module and closure member are fixed together by the mode with sealing then.Under the situation of glass/silicon stone element, carry out seal operation by melting element, and under the situation of hardware, by element is welded together or by element peripheral insert one or more liners of making by material and for example described element be linked together by being threaded with chemoresistance realize seal operation.These assembling process costlinesses, consuming time, and need on the one hand to use auxiliary equipment (for example smelting furnace, welding equipment), and need FA manufacturing technology on the other hand.In addition, if passage need be cleaned, these reactors of great majority can not be opened under situation about not being destroyed, or take apart very complicated.
In addition, do not handle the conduit wall out-of-flatness on microcosmic (just " thin texture/granular texture being arranged ") that forms through additional surface by said method, this will form relatively large surface.Therefore, conduit wall can suffer the reactant of violent effect, as the invasion and attack of ozone, perhaps under special circumstances, the structure of wall can cause any reaction intermediate or even reactant (ozone) itself be decomposed uncontrollablely.
Summary of the invention
Therefore, the objective of the invention is to eliminate the shortcoming of present normally used micro-fluidic reactor above-mentioned or it is improved.Especially, a purpose of the present invention provides a kind of method that forms the seal channel of micro-fluidic reactor, this method need not to use auxiliary devices, and can also make the micro-fluidic reactor that has high resistance for the active reaction thing cheap and simply in addition.Another object of the present invention provides a kind of method, wherein, when reactor module and closure member are fixed together by being threaded, need to the sealing of passage with in reactor module, form passage and carry out simultaneously---in same manufacturing step.Another purpose of the present invention provides a kind of micro-fluidic reactor, when this micro-fluidic reactor of assembling, do not need independent seal operation to passage, wherein, the reactor that assembles can react on a large scale, particularly is accompanied by the reaction that a large amount of heats produce---in temperature on a large scale and temperature that can the quick adjustment passage.
In one aspect of the invention, above-mentioned purpose is achieved by a kind of method that forms seal channel in the sheet surface of being made by the material with plasticity to a certain degree is provided, and this method comprises the steps: to make first point of the passage that a machining surface contact with instrument of roller press finished surface will form in the surface of the thin slice of anabolic reaction device module; Utilization causes the required pressure of the degree of depth of the passage that will form that described machining surface is pressed into described sheet surface, thereby plastic material is extruded, and along the periphery of the recess that is forming from the sheet surface projection; When keep-uping pressure, by machining surface is rolled to from first of the passage that will form described machining surface is moved at second at sheet surface along the center line of passage, machining passage in the material of thin slice thus, and along the periphery of passage by being extruded and the material of projection forms sealing strip; Surface at the thin slice that is provided with passage and sealing strip is provided with closure member, to bear against described sealing strip; With making the required pressure of described sealing strip deformation be pressed in described closure member on the thin slice and being fixed in resulting position, be extended with seal channel between first and second in being formed at reactor module thus.
Experience shows, is extruded along the periphery of resulting passage and the plastic material that protrudes is particularly useful for providing the sealing with high anti-patience, and this is considered to surprising and not expectable effect.The thickness range of the material that is extruded is 10 to 200 μ m, and the material that is extruded provides durable especially this fact of sealing to be owing to cause the increase of the shearing that material is extruded to cause the surprising of material and not expectable structural change.
Other preferred embodiment of the method according to this invention is disclosed in dependent claims 2-8.
In still another aspect of the invention, above-mentioned purpose realizes by a kind of micro-fluidic reactor is provided, in this micro-fluidic reactor, passage extends as the recess of the one side of anabolic reaction device module, described the face that contacts with first stopper with reactor module is relative, wherein, the periphery of passage is by delimiting from the zone that forms sealing strip that the face of reactor module stretches out by deformation, closure member is forced into channelled of reactor module, thereby make described closure member bear against sealing strip, temperature conditioning unit be forced into closure member with the sealing strip facing surfaces.
Preferred embodiment according to micro-fluidic reactor of the present invention is disclosed in dependent claims 10-17.
Description of drawings
Describe the present invention in detail below with reference to accompanying drawing, wherein:
Fig. 1 is the front view that includes partial sectional view according to an embodiment of micro-fluidic reactor of the present invention;
Fig. 2 is the top view of the micro-fluidic reactor shown in Fig. 1;
Fig. 3 is the cutaway view of the micro-fluidic reactor A-A along the line shown in Fig. 1;
Fig. 4 is the bottom view of the micro-fluidic reactor shown in Fig. 1;
Fig. 5 A shows according to the passage of micro-fluidic reactor of the present invention and preferably uses in the forming process of spherical machinery tools cutaway view perpendicular to flow direction at it;
Fig. 5 B shows the cutaway view perpendicular to flow direction of completed passage in the micro-fluidic reactor that assembles; With
Fig. 6 is the schematic diagram according to another embodiment of micro-fluidic reactor of the present invention.
The specific embodiment
Fig. 1 shows micro-fluidic reactor 100, the closure member 130 on second 120B that it comprises the reactor module 120 that is limited by first 120A and second 120B, first limited part 110 that contacts with first 120A of reactor module 120, be covered in reactor module 120, with closure member 130 along second limited part 160 on its peripheral supporting member 140 that contacts and the face relative that be resisted against supporting member 140 with closure member 130.Closure member 130, supporting member 140 and limited part 160 define a cooling chamber 153 together between them.The temperature conditioning unit 150 that contacts with closure member 130 is installed in cooling chamber 153.Temperature conditioning unit 150 passes through supporting member 140 installation in position securely.In this layout, temperature conditioning unit 150 separates a gap with second limited part 160, that is to say, the temperature conditioning unit 150 and second limited part 160 are not in contact with one another.Cooling chamber 153 is communicated with external environment condition by the preferably threaded through hole 167,169 that is formed in second limited part 160.
Described first and second limited parts 110,160 are used for keeping together and protecting them to avoid exterior mechanical and impact being arranged on element between them.Therefore, limited part 110,160 is made by the steel with high mechanical strength, for example stainless steel.Limited part 110 also is provided with the through hole (not shown), to allow external environment condition and the channel connection that is formed in the reactor module 120.These through holes preferably are adapted to sealing and releasable mode and admit the example threaded through hole of connector 180,182,184 as shown in Figure 2.One of through hole 167,169 is admitted the cryogen organization of supply 157 that leads to flow channel 155, and described flow channel 155 is limited by the gap of the temperature conditioning unit 150 of contiguous reactor 100.Described cryogen organization of supply 157 is admitted with sealing and releasable mode.Being tightly connected of cryogen organization of supply 157 provides by the liner 158 that is arranged between limited part 160 and the cryogen organization of supply 157 self.Liner 158 preferably forms O shape ring.Be formed in the threaded through hole 167,169 in the limited part 160 another and be adapted to sealing and releasable mode and admit a cryogen output mechanism 159, wherein, described cryogen output mechanism 159 opens wide from described gap 155.Being tightly connected of cryogen output mechanism 159 provides (not shown) by the liner that is arranged between limited part 160 and the cryogen output mechanism 159 self, and wherein, this liner preferably forms O shape ring.
The embodiment of passage 125 shown in Figure 3 comprises respectively the paths 190,192,194 that flow and be communicated with connector 180,182,184.In the present embodiment, path 190,192 is used to supply reactant, and path 194 is used for discharging the product of the chemical reaction that carries out at reactant mixture, and described reactant mixture obtains by the hybrid element 129 that is attached in the passage 125.In the present embodiment, hybrid element 129 is formed by the Y shape connector that is arranged in the passage 125.The length of the portion section of passage 125 between hybrid element 129 and path 194 is selected such that, the chemical reaction of the hope of the reactant that is in contact with one another by hybrid element 129 carried out before reactant arrives path 194.As shown in Figure 3, for helping the design of undersized reactor 100, passage 125 comprises parallel relatively long portion's section of extending and relative short portion's section of extending perpendicular to the former.Another advantage of this topological structure of passage 125 is that owing to the big ratio of channel surface with respect to channel volume, the temperature of reactants/reaction mixture can be changed fast and reliably.Certainly, the shape of passage 125 can be with shown different.For example, passage 125 can comprise the spiral branch that joins in the hybrid element 129, and the temperature controlled advantage of remaining valid simultaneously.
Shown in Fig. 5 B, passage 125 forms in face 120B in the following manner: after clamping reactor module 120 suitably, by the F that exerts pressure with the machinery tools with roller press finished surface, be preferably spherical machinery tools 80 and be pressed onto on the face 120B, described pressure F selects according to the material and the plasticity of reactor module 120, wherein, according to program described roller press finished surface of guiding in a guiding (or control) that is placed on limited part 110 places is installed.The value of applied pressure F is chosen to make that the ball 85 of machinery tools 80 inwardly protrudes in the body of reactor module 120, the feasible whole hope degree of depth that forms passage 125 of its degree.Then, move forward spherical machinery tools 80 according to suitable adjusting continuously along the predefined paths of required passage 125 and form passage 125, wherein, move forward speed and be generally 0.1-5mm/s control.Continuous moving forward between moving period at machinery tools 80 with roller press finished surface, the material of reactor module 120 becomes fine and close also owing to the shearing that produces is extruded along the periphery of passage 125, its result makes and forms a sealing strip 127 along each relative periphery of passage 125, described sealing strip 127 is parallel to passage and extends, shown in Fig. 5 B.The size of passage 125 and sealing strip 127 depends on the diameter of the machining surface of machinery tools.When using described spherical machinery tools 80, the diameter of the ball 85 that the size of the width of passage 125 and the sealing strip 127 that forms with passage 125 can be by changing machinery tools 80 is adjusted.The degree of depth of passage 125 can be by changing spherical machinery tools 80 the height and position of ball 85 adjust.Those skilled in the art can be obvious, the special spherical machining surface that replaces ball 85 to provide, other machining surface, also applicable as cylindrical surface.
Under the situation of manual formation passage 125, at first by on face 120B, marking the trace that trace comes mark channel 125.But, forming in mechanization under the situation of passage 125, the trace of hope is stored in the device of the spherical machinery tools 80 of guiding preferably as numerical data.
By closure member 130 being set on face 120B or on outstanding thereon the sealing strip 127 and the passage 125 that is formed in the reactor module 120 being sealed by exerting pressure perpendicular to the plane of closure member 130.Because the power that applies, sealing strip 127 produces deformation, thereby causes the sealed engagement between reactor module 120 and the closure member 130.Should be noted that in this case pressure only is distributed on the sealing strip 127 of face 120B, rather than on whole 120B, this causes sealing more reliably.For closure member 130, use is made by the material with thermal conductive resin and chemoresistance, ganoid sheet shaped piece/film of while.If thermal conductive resin is necessary, then closure member 130 is made by the PTFE film that thickness is 20 μ m to the maximum.
Behind seal channel 125, be that reactor module 120 is provided with through hole along the thickness of reactor module 120 at path 190,192,194 places, so that connector 180,182,184 is communicated with path 190,192,194 respectively.
Preferably, supporting member 140 is the form of aluminum square box.
The temperature conditioning unit 150 that is contained in the supporting member 140 is installed in the facing surfaces place of closure member 130 with respect to passage 125, is positioned to contact with closure member 130, as shown in Figure 1.One preferred embodiment of temperature conditioning unit 150 preferably is arranged to tandem type Peltier unit (comprise a plurality of but be preferably two Peltier elements that are in contact with one another), and it is operated based on Peltier effect.Can be obvious as those skilled in the art, Peltier element is a kind of device that comprises two thin ceramic sheets and therebetween a plurality of wafers, when when this device applies suitable electric current and voltage, will between its both sides, provide stationary temperature poor.In its simplest form, there are two different metal levels in the bottom side of Peltier element, electric current passes through wherein to flow, thereby causes the hot-fluid between the metal level.Therefore obtain a cold side and a warm side.Be used in according to the cold side of first Peltier element 151 of the temperature conditioning unit 150 in the micro-fluidic reactor 100 of the present invention and contact by closure member 130 and reactor module 120 or the reactants/reaction mixture that is contained in the passage 125.Simultaneously, the warm side that is used in first Peltier element 151 of the temperature conditioning unit 150 in the micro-fluidic reactor 100 contacts with the cold side of second Peltier element 152.Be used for controlling according to the temperature conditioning unit 150 of the temperature of reactor 100 an of the present invention body unit by described two Peltier elements 151,152 form, preferably at a shared leg (casing).Contact with the warm side of first peltier-element 151 and therefore also with second peltier-element 152 of its cooling more than first peltier-element 151 effective force more.
In reactor 100 according to the present invention, the heat that produces in the warm side of more virtuous second peltier-element 152 is removed by cooling, and cryogen is used to described cooling.Cryogen is infeeded in the coolant flow channel 155 that is arranged between temperature conditioning unit 150 and the limited part 160 by cryogen organization of supply 157.Cryogen is therefrom discharged by cryogen output mechanism 159.For described cryogen, preferably make water.Autoreactor 100 inside lead to and are used to operate the required electric conductor (not shown) of the temperature conditioning unit that formed by two peltier-element 151,152 150 between closure member 130 and supporting member 140.Utilization is used in according to the temperature conditioning unit 150 in the reactor 100 of the present invention, if thermic load is zero, then the temperature difference between passage 125 and the external environment condition can reach even 70 ℃.Not being that the maximum temperature difference of passage 125 is less certainly under zero the situation in thermic load, for example, is that the temperature of passage 125 can reach-50 ℃ approximately under 25 ℃ the situation for+5W, ambient temperature in thermic load.In addition, utilize temperature conditioning unit 150 to be approximately 8 ℃/s (in 0 to 20 ℃ of scope) by thin closure member 130 available maximum temperature rate of change in passage 125.For a person skilled in the art, obviously,, can use the heating/cooling way of other type except tandem type temperature conditioning unit 150 with being equal to.
Keep by suitable coupling mechanism and be clamped together according to the closure member 130 of first limited part 110 of micro-fluidic reactor 100 of the present invention, reactor module 120, temperature conditioning unit 150 and supporting member 140, with in 130 formation of reactor module 120 and closure member and the sealings that remain intact.In the embodiment shown in fig. 1, coupling mechanism forms by through bolt 170 and the nut of tightening thereon 172, and described through bolt is plugged in the through hole (unmarked) that is formed in each described part and crosses over the whole thickness of reactor 100.For a person skilled in the art, obviously, the described part of each of reactor 100 also can be clamped together by other coupling mechanism, for example by the spring locking mechanism.In addition, the quantity that should be noted that the connection element of used coupling mechanism can change according to the shape (rectangle, square, circle etc.) of the plane projection of reactor 100.For example, under the situation of the reactor shown in Fig. 2-4 100, reactor 100 has the square-shaped planar projection, uses four through bolts 170 to guarantee the clamping of suitable degree.
After utilizing spherical machinery tools 80 formation passages 125 and sealing strip 127, assemble as follows according to micro-fluidic reactor 100 of the present invention.At first, described through bolt 170 is inserted in the through hole that is arranged in the limited part 110, then reactor module 120 is arranged on the limited part 110, make its face 120A towards limited part 110.Next, closure member 130 is put on the sealing strip 127 among the face 120B that is formed on reactor module 120.In following step, with supporting member 140 be placed on its inner temperature conditioning unit 150 in advance and be placed on together on the surface of closure member 130, relative with passage 125; After being set to limited part 160 on the through bolt 170, be clamped together by each the described part that nut 172 is tightened on the through bolt 170 reactor 100.By nut 172 being tightened to the joint that utilizes on the through bolt 170 between sealing strip 127 seal channels 125 and the closure member 130.At last, connector 180,182,184 is fixed in the through hole of limited part 110 and cryogen organization of supply 157 and cryogen output mechanism 159 is fixed to the through hole separately 167,169 of limited part 160.
Fig. 6 shows another the possible preferred embodiment according to micro-fluidic reactor 200 of the present invention.Reactor 200 is different from reactor shown in Figure 1 100 on connecting mode, that is, under the situation of reactor 100, be threaded togather and closure member 130 is pressed onto sealing strip 127 by the each several part with reactor 100; And here, pressure provides by vacuum.
As shown in Figure 6, micro-fluidic reactor 200 comprise reactor module 220, with face contact of reactor module 220 and extend beyond its periphery first limited part 210, cover reactor module 220 the face relative with limited part 210 closure member 230 and towards second limited part 260 of first limited part 210.By carrying out the method according to this invention recited above, reactor module 220 form passage in the surface of closure member 230 and along the sealing strip (all not illustrating in the drawings) of this passage.A side relative with reactor module 220 of closure member 230 is provided with the temperature conditioning unit 250 with the described side contacts of closure member 230.In the present embodiment, reactor module 220, closure member 230 disposed thereon have formed the reactor core 223 with given crosswise yardstick with the temperature conditioning unit 250 that contacts with closure member 230.Second limited part 260 is adapted to admits reactor core 223.Limited part 260 has the profiled outline that comprises the section that is limited by first step 281 and second step 283 towards the surface of first limited part 210.
In the zone of the near surface of limited part 210, be formed with groove 285 at limited part 260.In groove 285, be plugged with seal 288.The surface of step 281 is provided with the seal 289 that extends in the form of a ring in limited part 260.
The micro-fluidic reactor that assembles 200 is the seal 288 in the groove 285 that is arranged on first limited part 210 on the one hand, on the other hand against the seal 289 of temperature conditioning unit 250.Therefore, first limited part 210, second limited part 260 and reactor core 223 define enclosed cavity 287 together.This enclosed cavity 287 communicates with external environment condition via the through hole 293 that is formed on the preferred threaded in first limited part 210.In special circumstances, through hole 293 is adapted to sealing and releasable mode and admits the vacuum coupling 286 that is equipped with plug valve.Vacuum coupling 286 links to each other with suitable vavuum pump (not shown).Temperature conditioning unit 250 and limited part 260 define the flow channel 255 that is used for refrigerant cycle together.Flow channel 255 is communicated with external environment condition is mobile via the through hole 267,269 that is formed in second limited part 260.Seal 288,289 is preferably made by rubber or other material with given flexibility.
Energize for the vavuum pump that is connected to vacuum coupling 286 and in chamber 287, to cause vacuum, thereby overcome the maintenance effect of seal 288,289 and first and second limited parts 210,260 are pulled to each other.As a result, push temperature conditioning unit 250 to closure member 230 at the pressure that seal 288 places cause, this closure member then be pressed towards the sealing strip that is formed in the reactor module 220, this causes the intact sealing of passage.After in chamber 287, reaching the vacuum of predetermined extent, will make closure member 230 press the power that is formed on the sealing strip on the reactor module 220 by the plug valve of closing vacuum coupling 286 and be set at steady state value.If desired, plug valve can be opened, and makes level of vacuum (with therefore pressure size) keep constant with operated vacuum pumps once more.
The connection based on vacuum that is used for micro-fluidic reactor 200 causes the even distribution of the power on sealing strip, and this has further improved the sealing of the passage that is used to provide reaction compartment.
In the preferred embodiment of micro-fluidic reactor 100,200 according to the present invention, all surfaces that is used to form the Flow Control structure is 25cm
2Passage length is 65mm, the average diameter of passage is 400 μ m, the degree of depth of passage also is 400 μ m, and the quantity of import and outlet is 3, uses single hybrid element, the accessible minimum temperature of passage is-50 ℃ (in thermic loads during for+5W), the accessible maximum temperature of passage is 150 ℃, and the maximum operating pressure of reactor is 30 crust, and the maximum rate of change of temperature is 8 ℃/s (in 0 to 20 ℃ a scope).Should be understood that according to specific reaction micro-fluidic reactor 100,200 according to the present invention can have different yardsticks, have different hybrid element quantity and different import and export volumes.
Micro-fluidic reactor 100,200 according to the present invention is particularly useful for carrying out various ozonolysis reactions, as describing in the example below, because in this reaction that occurs in heterogeneous (gas/liquid), the size of the value of time of contact and control ability and contact surface is very crucial.In addition, because these exothermic heat of reaction are necessary with shifting reliably with reaction heat fast, this will significantly be strengthened by being arranged on according to the passage of micro-fluidic reactor of the present invention and the extremely thin closure member between heating/cooling unit.In order to keep control to ozonolysis reactions, promptly, in order to control reactivity, for most of this reactions keep reaction temperatures to be lower than environment temperature and the subsequent chemistry process of the intermediate product (ozonide) that obtains for ozonolysis reactions the environment of cooling is provided is necessary.In addition, the very unstable and therefore very easily blast of ozonide.
Example
Is that the solution (1: 1) of 5-methyl isophthalic acid-H-indoles in methyl alcohol/dichloro methyl alcohol of 0.025mol/l is introduced in the passage 125 according to micro-fluidic reactor 100 of the present invention by connector 180 and path 190 with concentration, is that the ozone of constant basis of 5% volume and the gaseous mixture of oxygen are introduced in the passage 125 with by volume by connector 182 and path 192 simultaneously.The flow rate of the 5-methyl isophthalic acid-H-indoles solution by reactor 100 is constant to be 0.25ml/min, wherein, remains the pressure of 5 crust in whole process in reactor 100.Be reflected under 0 ℃ of the temperature and carry out.To drip to the NaBH the mixture (1: 1) that is suspended in methyl alcohol and dichloroethanes by the product that path 194 and connector 184 are discharged from reactor 100
4On (borohydride sodium).This second reactant (is NaBH
4) guarantee the decomposition of the intermediate product (ozonide of generation) that reacts.Especially, intermediate product can be decomposed in having second (micro-fluidic) reactor of similar structures equally.The magnitude of the mean residence time in reactor 100 is second.Product is N-(2-methylol-4-aminomethyl phenyl) formamide.Analyze according to HPLC (high performance liquid chromatography), the purity of product is 98%.
The output of the reaction of carrying out in traditional reactor is that about 60-65% is (for example with reference to Journalof the Chemical Society (1953) 3440-3443 pages or leaves, perhaps Journal of theChemical Society (1950) 612-618 pages or leaves), this is mainly from the unmanageable reaction condition and the ratio of therefore coming self-reacting accessory substance.Under the situation of reacting when improvement of terms the time, output reduces pro rata with the increase of purity, that is, when degree of purity of production increased, productivity ratio reduced pro rata.
Summary: under situation according to micro-fluidic reactor of the present invention, required heat transmission provides in the following way: the reactant mixture in the passage is contacted with cooling unit by the extremely thin PTFE film that a thickness is approximately 20 μ m, and described passage has a relatively large surface/volume.In addition, according to the manufacturing of the micro-fluidic reactor of the present invention manufacturing technology of needs costliness not, because the sealing to passage can simple and cheap mode realize---be connected to the reactor part by making that by means of for example through bolt or vacuum the sealing strip that utilizes spherical machinery tools to form with passage is stressed, and under their coupled situation, they fixed then.In addition, in order to clean, can be by outwarding winding attachment bolt or take apart simply according to micro-fluidic reactor of the present invention by discharging vacuum, after finishing cleaning course, micro-fluidic reactor can be assembled once more.Other advantage of the present invention is, in channel geometry optimization and/or manufacturing exemplar stage, also can easily and apace carry out uniqueness and the change subsequently of channel of reactor.
Claims (17)
1. method that in the surface of the thin slice of anabolic reaction device module, is formed for the seal channel (125) of micro-fluidic reactor, described thin slice is made by the material with plasticity to a certain degree, it is characterized in that, and this method comprises the steps:
(a) machining surface with instrument of roller press finished surface being contacted will be in anabolic reaction device module (120; First point of the passage that forms in the surface of thin slice 220) (125);
(b) utilizes and to cause the required pressure (F) of the degree of depth of the passage (125) that will form that described machining surface is pressed into described sheet surface, thereby plastic material is extruded, and along the periphery of the recess that is forming from the sheet surface projection;
(c) in keep-up pressure (F), by machining surface is rolled to from first of the passage (125) that will form described machining surface is moved at second at sheet surface along the center line of passage (125), machining passage (125) in the material of thin slice thus, and along the periphery of passage (125) by being extruded and the material of projection forms sealing strip (127);
(d) in the surface of the thin slice that is provided with passage (125) and sealing strip (127) closure member (130 is set; 230), to bear against described sealing strip (127);
(e) with making the required pressure of described sealing strip (127) deformation with described closure member (130; 230) be pressed on the thin slice and be fixed in resulting position, be formed at reactor module (120 thus; 220) extend seal channel (125) between first and second in.
2. according to the described method of claim 1, it is characterized in that described roller press finished surface is columniform.
3. according to the described method of claim 1, it is characterized in that described roller press finished surface is spherical.
4. according to the described method of claim 3, it is characterized in that described spherical machining surface provides by the surface of ball (85).
5. according to the described method of claim 1, it is characterized in that from the difference of thin slice, repeating step (a) is to (c), up to the channel design that obtains to wish pattern.
6. according to the described method of claim 1, it is characterized in that, by at the end points place of passage (125) to reactor module (120; 220) boring comes at reactor module (120; 220) form outlet and at least one import in the face (120A), described outlet and at least one import are all flowed with passage (125) and are communicated with described (120A) and reactor module (120; 220) the face that has passage (125) (120B) is relative.
7. according to the described method of claim 1, it is characterized in that described reactor module (120; 220) thin slice is made by the plastic material with chemoresistance, is preferably made by plastic material that fluoridize and/or chlorination, is more preferably made by polytetrafluoroethylene (PTFE).
8. according to the described method of claim 1, it is characterized in that, make the required pressure of sealing strip (127) deformation utilize vacuum to provide.
9. micro-fluidic reactor that comprises the seal channel that is used to hold chemical reaction, described passage is provided with import and outlet is communicated with the external environment condition of reactor being used for, described reactor also comprises by coupling mechanism maintenance and first and second limited parts that are clamped together, is arranged on reactor module, closure member between the described limited part and the cooling chamber that is communicated with the external environment condition of reactor, wherein, in described cooling chamber, be provided with temperature conditioning unit, it is characterized in that described passage (125) is as anabolic reaction device module (120; The recess of face 220) (120B) extends, described (120B) and reactor module (120; 220) with first limited part (110; 210) Jie Chu face (120A) is relative, wherein, the periphery of passage (125) by by deformation from reactor module (120; Delimit in the zone of the formation sealing strip (127) that face 220) (120B) stretches out; Closure member (130; 230) press reactor module (120; 220) the face with passage (125) (120B), thus described closure member (130 made; 230) bear against sealing strip (127); Temperature conditioning unit (150; 250) press closure member (130; 230) with sealing strip (127) facing surfaces.
10. micro-fluidic reactor according to claim 9 is characterized in that, described reactor module (120; 220) and closure member (130; 230) make by material with chemoresistance.
11. micro-fluidic reactor according to claim 10 is characterized in that, described reactor module (120; 220) make by plastic material, preferably make, more preferably make by polytetrafluoroethylene (PTFE) by plastic material that fluoridize and/or chlorination with chemoresistance.
12. micro-fluidic reactor according to claim 10 is characterized in that, described closure member (130; 230) the polytetrafluoroethylene (PTFE) film that is 20 μ m to the maximum by thickness is made.
13. micro-fluidic reactor according to claim 9 is characterized in that, described temperature conditioning unit (150; 250) form tandem type amber ear card unit.
14. micro-fluidic reactor according to claim 13 is characterized in that, described tandem type amber ear card unit comprises first Peltier's element (151) and second Peltier's element (152), and they are arranged in the shared leg and are in contact with one another.
15. micro-fluidic reactor according to claim 9 is characterized in that, is being positioned at temperature conditioning unit (150; 250) with closure member (130; 230) be formed with coolant flow channel (155 in the cooling chamber in the facing surfaces (153); 255).
16. micro-fluidic reactor according to claim 9, it is characterized in that, described second limited part (260) is arranged to first limited part (210) and is divided relative by the reactor section that reactor core (223) forms, described reactor core comprises reactor module (220), closure member disposed thereon (230) and press the temperature conditioning unit (250) of closure member (230), described second limited part (260) is adapted to a sideshake and admits reactor core (223), wherein, between first limited part (230) and second limited part (260), and between reactor core (223) and second limited part (260), be plugged with separately seal (288,289), chamber (287) to be used to be provided for vacuum.
17. micro-fluidic reactor according to claim 16 is characterized in that, described chamber (287) are communicated with external environment condition via the through hole (293) that is formed in first limited part (210), and described chamber (287) are adapted to and admit vacuum coupling (286).
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| HUP0501205 | 2005-12-23 | ||
| HU0501205A HU227586B1 (en) | 2005-12-23 | 2005-12-23 | Method for forming sealed channel of microfluidical reactor and microfluidical reactor containing the same |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101360680A true CN101360680A (en) | 2009-02-04 |
Family
ID=89986491
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2006800516610A Pending CN101360680A (en) | 2005-12-23 | 2006-12-22 | Method of forming a sealed channel of a microfluidic reactor and a microfluidic reactor comprising such channel |
Country Status (10)
| Country | Link |
|---|---|
| US (1) | US7919055B2 (en) |
| EP (1) | EP1971548A2 (en) |
| JP (1) | JP2009520597A (en) |
| CN (1) | CN101360680A (en) |
| AU (1) | AU2006327903A1 (en) |
| HU (1) | HU227586B1 (en) |
| IL (1) | IL192392A0 (en) |
| NO (1) | NO20083196L (en) |
| RU (1) | RU2008129186A (en) |
| WO (1) | WO2007072099A2 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111194240A (en) * | 2017-10-06 | 2020-05-22 | 康宁股份有限公司 | Flow reactor fluid coupling apparatus and method |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2011104554A (en) * | 2009-11-20 | 2011-06-02 | Nisso Engineering Co Ltd | Microreactor |
| JP2013208619A (en) * | 2013-06-21 | 2013-10-10 | Nisso Engineering Co Ltd | Microreactor |
| US9861982B2 (en) * | 2015-03-09 | 2018-01-09 | Emd Millipore Corporation | Connectors for pneumatic devices in microfluidic systems |
| US10376885B2 (en) * | 2015-11-04 | 2019-08-13 | Lehigh University | Microfluidic concentrator for label-free, continuous nanoparticle processing |
Family Cites Families (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4413407A (en) | 1980-03-10 | 1983-11-08 | Eastman Kodak Company | Method for forming an electrode-containing device with capillary transport between electrodes |
| US5201996A (en) | 1990-04-30 | 1993-04-13 | Bell Communications Research, Inc. | Patterning method for epitaxial lift-off processing |
| SE9100392D0 (en) | 1991-02-08 | 1991-02-08 | Pharmacia Biosensor Ab | A METHOD OF PRODUCING A SEALING MEANS IN A MICROFLUIDIC STRUCTURE AND A MICROFLUIDIC STRUCTURE COMPRISING SUCH SEALING MEANS |
| US5534328A (en) | 1993-12-02 | 1996-07-09 | E. I. Du Pont De Nemours And Company | Integrated chemical processing apparatus and processes for the preparation thereof |
| EP0695941B1 (en) | 1994-06-08 | 2002-07-31 | Affymetrix, Inc. | Method and apparatus for packaging a chip |
| WO2001009598A1 (en) * | 1999-07-28 | 2001-02-08 | University Of Washington | Fluidic interconnect, interconnect manifold and microfluidic devices for internal delivery of gases and application of vacuum |
| DE10106952C2 (en) * | 2001-02-15 | 2003-01-16 | Cognis Deutschland Gmbh | Chip reactor |
| US7060227B2 (en) | 2001-08-06 | 2006-06-13 | Sau Lan Tang Staats | Microfluidic devices with raised walls |
| JP4804718B2 (en) | 2003-04-28 | 2011-11-02 | 富士フイルム株式会社 | Fluid mixing device and fluid mixing system |
| US7223949B2 (en) | 2004-04-21 | 2007-05-29 | Beckman Coulter, Inc. | Analysis apparatus having improved temperature control unit |
-
2005
- 2005-12-23 HU HU0501205A patent/HU227586B1/en not_active IP Right Cessation
-
2006
- 2006-12-22 US US12/158,784 patent/US7919055B2/en not_active Expired - Fee Related
- 2006-12-22 CN CNA2006800516610A patent/CN101360680A/en active Pending
- 2006-12-22 AU AU2006327903A patent/AU2006327903A1/en not_active Abandoned
- 2006-12-22 EP EP06831526A patent/EP1971548A2/en not_active Withdrawn
- 2006-12-22 RU RU2008129186/28A patent/RU2008129186A/en unknown
- 2006-12-22 JP JP2008546655A patent/JP2009520597A/en active Pending
- 2006-12-22 WO PCT/HU2006/000127 patent/WO2007072099A2/en active Application Filing
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2008
- 2008-06-23 IL IL192392A patent/IL192392A0/en unknown
- 2008-07-17 NO NO20083196A patent/NO20083196L/en not_active Application Discontinuation
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111194240A (en) * | 2017-10-06 | 2020-05-22 | 康宁股份有限公司 | Flow reactor fluid coupling apparatus and method |
| CN111194240B (en) * | 2017-10-06 | 2022-09-06 | 康宁股份有限公司 | Flow reactor fluid coupling apparatus and method |
Also Published As
| Publication number | Publication date |
|---|---|
| EP1971548A2 (en) | 2008-09-24 |
| AU2006327903A1 (en) | 2007-06-28 |
| WO2007072099A3 (en) | 2007-09-13 |
| US7919055B2 (en) | 2011-04-05 |
| HU227586B1 (en) | 2011-08-29 |
| HUP0501205A2 (en) | 2007-07-30 |
| NO20083196L (en) | 2008-09-11 |
| US20090098029A1 (en) | 2009-04-16 |
| IL192392A0 (en) | 2008-12-29 |
| RU2008129186A (en) | 2010-01-27 |
| HU0501205D0 (en) | 2006-02-28 |
| JP2009520597A (en) | 2009-05-28 |
| WO2007072099A2 (en) | 2007-06-28 |
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